CN110014145B - Preparation method of spherical ferrite-based powder - Google Patents
Preparation method of spherical ferrite-based powder Download PDFInfo
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- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
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- C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/50—Ferrous alloys, e.g. steel alloys containing chromium with nickel with titanium or zirconium
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/58—Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.5% by weight of manganese
Abstract
The invention belongs to the field of preparation research of spherical metal-based powder, and particularly provides a preparation method of spherical ferrite-based powder co-reinforced by intermetallic compounds and nano oxides. The method comprises the following steps: preparing a precursor slurry; preparation of intermetallic compound and nano-oxide co-reinforced spherical ferrite-based powder product: and carrying out radio frequency plasma spheroidization on the obtained precursor slurry, conveying the precursor slurry to an atomizing nozzle by carrier gas, atomizing the precursor slurry, then enabling the atomized precursor slurry to reach a high-temperature region heated by radio frequency plasma, decomposing nitrate to obtain corresponding oxide nano particles, heating and melting the atomized powder and the oxide nano particles by the radio frequency plasma, and then changing the atomized powder and the oxide nano particles into spherical ferrite-based powder under the action of surface tension. The invention provides a new idea for preparing intermetallic compound and nano oxide co-reinforced spherical ferrite-based powder, and has the advantages of short production period, low cost, convenient operation and the like.
Description
Technical Field
The invention belongs to the field of preparation research of spherical metal-based powder, and particularly provides a preparation method of spherical ferrite-based powder.
Background
The ferrite alloy co-strengthened by the intermetallic compound and the nano oxide has a gamma/gamma' coherent two-phase structure similar to that of a nickel-based alloy, is expected to improve the service temperature limit and the high-temperature mechanical property of the traditional ferrite alloy, and has important application prospect in the field of high-temperature structural materials.
Generally, the ferrite-based alloy mainly comprises Fe, Cr, Ni, Al, Mn, Ti and Mo, wherein Fe is the main component element of the ferrite of the alloy matrix. The addition of a proper amount of Cr is beneficial to improving the corrosion resistance of the alloy, and meanwhile, the Cr is dissolved in the matrix to achieve the solid solution strengthening effect. Ni and Al are mainly forming elements of intermetallic compound NiAl (beta'), are main second phases in the alloy and play a role in strengthening precipitation in the alloy. Recent research shows that the plasticity of the alloy is greatly reduced by excessively high content of the Al element, and the addition of a small amount of Mn element in the alloy can occupy the position of the Al element in NiAl, so that the dependence of the alloy on the Al element can be reduced, and the plasticity of the alloy can be improved without losing the strength of the alloy (Acta Materialia, 2015, 84: 283-. The addition of Mo also can play a role in solid solution strengthening, and can increase the lattice constant of a ferrite matrix. This can further reduce the lattice mismatch of the beta 'precipitate phase and the ferrite matrix, thereby reducing the potential barrier for beta' precipitation and increasing the nucleation rate thereof during aging. Since the NiAl strengthening phase is easy to destabilize and coarsen at high temperature, a certain amount of Ti element is often introduced into the alloy to generate Ni through heat treatment2An AlTi phase. Addition of an appropriate amount of Ti will result in Ni2The AlTi phase tends to wrap the NiAl phase heterogeneous nucleation to form composite precipitated particles, thereby effectively reducing the medium-high temperature diffusion capability of the NiAl phase, inhibiting the coarsening of the NiAl phase and obviously improving the medium-high temperature creep resistance of the alloy (Acta Materialia, 2017,127: 1-16). In addition, Ti is also a strong carbide forming element, and is matched with a proper process to be finely dispersedThe carbide can effectively improve the alloy strength.
The nano-oxide particles are the second important strengthening phase in the ferrite alloy in which the intermetallic compound is precipitated and strengthened and the nano-oxide is co-strengthened. The nanometer oxide particles generally have high thermal stability and can not be dissolved in a matrix at high temperature, so that the use temperature of the alloy can be effectively increased. Meanwhile, the nano-oxide particles with high volume fraction can effectively improve the radiation damage resistance and radiation swelling resistance (Journal of Nuclear Materials, 2017, 486: 11-20). Therefore, compared with the ferrite-based alloy reinforced by only using the intermetallic compound, the ferrite-based alloy co-reinforced by the intermetallic compound and the nano oxide has larger potential and wider possible application range.
The development of ferrite alloy reinforced by intermetallic compound and nano oxide and its advanced forming technology are the international research hot spots. Powder injection molding technology and 3D printing technology are taken as representative technologies of powder near-net shaping, and are suitable for shaping parts with moderate size and complex shapes. Because of a series of advantages of low cost, high precision, less cutting and even no cutting, the preparation of ferrite jointly reinforced by intermetallic compounds and nano oxides by the powder injection molding technology and the 3D printing technology attracts wide attention. In order to ensure the integrity of complex fine structures during near net shape forming, powders for powder injection molding and 3D printing generally require spherical powders to ensure their flowability and filling properties.
However, at present, most methods for preparing ferrite-based alloy powder reinforced by intermetallic compounds and nano-oxides are mechanical alloying methods. When the intermetallic compound and oxide jointly reinforced oxide dispersion reinforced ferrite-based alloy is prepared by the mechanical alloying process, Al, Ti, Mn and other elements are easy to be oxidized in the mechanical alloying process, so that NiAl and Ni are formed2The reduction of the intermetallic compound of AlTi cannot achieve the purpose of effectively controlling the amount of the intermetallic compound. Meanwhile, inclusions which are easily introduced by long-time ball milling can reduce the high-temperature mechanical property of the material. Finally, the powder obtained by mechanical alloying is mostly non-regular in shapeThe powder, the powder flowability is poor. This makes it impossible to perform near-net shape forming by methods such as 3D printing or powder injection molding. This severely limited the use of ferritic alloys with co-strengthening of intermetallic compounds and nano-oxides.
Disclosure of Invention
The invention aims to provide a method for preparing spherical ferrite-based powder with high designability, extremely fine oxide dispersed phase, high efficiency and superfine oxide dispersed phase.
The method comprises the steps of firstly preparing a powder precursor by adopting atomized powder of a target alloy and a corresponding oxide nitrate solution, then preparing the powder precursor into slurry with certain fluidity, and then spheroidizing the precursor slurry by using radio frequency plasma to obtain intermetallic compound and nano oxide co-reinforced spherical ferrite-based powder.
Accordingly, the present invention provides a method for preparing an intermetallic compound and nano-oxide co-strengthened spherical ferrite-based powder, the method comprising the steps of:
preparation of S1 precursor slurry: with Al (NO)3)3·9H2O、Y(NO3)2·6H2O and La (NO)3)2·6H2One of O is a nano oxide source, which is dissolved in a proper amount of solvent and then stirred to obtain a transparent solution, Fe- (6-14wt.%) Cr- (3-10wt.%) Ni- (1-3wt.%) Al- (0.5-4wt.%) Mn- (1-4wt.%) Ti- (1-5wt.%) Mo gas atomized powder is added into the transparent solution until the alloy powder is just soaked by alcohol, and the mixture is mixed for 0.5-4 hours at the rotating speed of 20-60 rpm by using a mixer to obtain a uniformly mixed precursor slurry, wherein the nano oxide source and the gas atomized powder are used in an amount which ensures that the nano oxide in the finally prepared powder accounts for 0.01-5wt.% of the mass percent of the ODS ferrite-based powder;
s2, preparation of the intermetallic compound and nano-oxide co-reinforced spherical ferrite-based powder product: and (2) carrying out radio frequency plasma spheroidization on the obtained precursor slurry, conveying the precursor slurry to an atomizing nozzle by carrier gas, atomizing, then reaching a high-temperature region heated by plasma, decomposing nitrate to obtain corresponding oxide nano particles, heating and melting the atomized powder and the oxide nano particles by the radio frequency plasma, then changing the atomized powder and the oxide nano particles into spheres under the action of surface tension, and cooling to obtain the intermetallic compound and nano oxide co-reinforced spherical ferrite-based powder.
In a specific embodiment, the solvent in S1 is an alcohol.
In a specific embodiment, the composition of the aerosolized powder in S1 is Fe- (6-14wt.%) Cr- (3-10wt.%) Ni- (1-3wt.%) Al- (0.5-4wt.%) Mn- (1-4wt.%) Ti- (1-5wt.%) Mo, wherein the Cr content is preferably 8-12 wt.%, the Ni content is preferably 4-8 wt.%, the Al content is preferably 1-2 wt.%, the Mn content is preferably 2-3 wt.%, the Ti content is preferably 2-3 wt.%, the Mo content is preferably 2-4wt.%, and the balance is Fe.
In one specific embodiment, the nano-oxide source in S1 is Al (NO)3)3·9H2O、Y(NO3)3·6H2O and La (NO)3)3·6H2And one of O, wherein the final nano oxide accounts for 0.01-5 wt%, preferably 0.1-1 wt% of the ODS ferrite-based powder.
In a specific embodiment, the carrier gas in S2 is argon, and the carrier gas flow is 1-10L/min, preferably 4-8L/min.
In a specific embodiment, the gas used in S2 is argon, and the flow rate of the gas is 15-40L/min, preferably 20-30L/min.
In a specific embodiment, the shell gas in S2 is argon, the shell gas flow is 65-100L/min, and the preferred shell gas flow is 70-80L/min.
In a specific embodiment, the precursor slurry feed rate in S2 is 20-200g/min, preferably 50-150 g/min.
In a specific embodiment, the negative pressure in the chamber in S2 is 6000-16000Pa, preferably 6500-13500 Pa.
The invention has the advantages and beneficial effects that:
1. the intermetallic compound and nano-oxide co-reinforced spherical ferrite-based powder obtained by the method has high sphericity, and the spherical powder has finer nano-scale oxide dispersed phase distributed therein.
2. The product prepared by the invention has strong designability, the product components are controllable, the particle size and the sphericity of the product can be controlled by a proper process, and the dispersed phase of the nano oxide is extremely fine.
3. The method has simple process, can directly obtain the spherical target powder from the precursor slurry, and is an efficient preparation method of the intermetallic compound and nano oxide co-reinforced spherical ferrite-based powder compared with a mechanical alloy and radio frequency plasma spheroidization method.
Drawings
Fig. 1 is a process flow diagram of a method for preparing spherical ferrite-based powder according to the present invention.
FIG. 2 is a schematic diagram of the preparation principle of intermetallic compound and nano-oxide co-reinforced spherical ferrite-based powder.
Detailed Description
The technical solution of the present invention is further described with reference to the following specific embodiments.
As shown in fig. 1, the present invention is a method for preparing a spherical ferrite-based powder, the method comprising the steps of,
preparation of S1 precursor slurry: dissolving a nano oxide source in a proper amount of solvent to obtain a transparent solution, adding gas atomized powder into the transparent solution for completely soaking, and mixing for 0.5-4 hours at the rotating speed of 20-60 revolutions per minute by using a mixer to obtain uniformly mixed precursor slurry;
preparation of S2 intermetallic compound and nano-oxide co-reinforced spherical ferrite-based powder product: and preparing the obtained precursor slurry into spherical ferrite-based powder by adopting a radio frequency plasma spheroidization technology, wherein the average grain diameter of an oxide dispersed phase in the spherical ferrite-based powder is less than or equal to 15 nm.
According to the embodiment of the present disclosure, the solvent in S1 is alcohol.
According to the embodiment of the disclosure, the nano-oxide source in S1 is Al (NO)3)3·9H2O、Y(NO3)3·6H2O or La (NO)3)3·6H2And O is one of the compounds.
According to the embodiment of the disclosure, the components of the aerosolized powder in S1 are: cr: 6-14wt.%, Ni: 3-10wt.%, Al: 1-3wt.%, Mn: 0.5-4wt.%, Ti: 1-4wt.%, Mo: 1-5wt.%, the balance being Fe.
According to the embodiment of the disclosure, each component of the aerosolized powder in S1 may also be: cr 8-12 wt.%, Ni4-8 wt.%, Al 1-2 wt.%, Mn 2-3 wt.%, Ti 2-3 wt.%, Mo 2-4wt.%, and the balance Fe.
According to the disclosed embodiment, the nano-oxide source in S1 is added in an amount ensuring that the nano-oxide accounts for 0.01-5wt.% of the total mass (referring to the mass of the final spherical ferrite-based powder) in the final spherical ferrite-based powder.
According to the disclosed embodiment, the nano-oxide source in S1 is added in an amount ensuring that the nano-oxide accounts for 0.1-1wt.% of the total mass (referring to the mass of the final spherical ferrite-based powder) in the final spherical ferrite-based powder.
According to the embodiment of the present disclosure, the specific process parameters of the radio frequency plasma spheroidization technique in S2 are as follows: the carrier gas is argon, the carrier gas flow is 1-10L/min, the middle gas flow is argon, the middle gas flow is 15-40L/min, the shell gas is argon, and the shell gas flow is 65-100L/min; the feeding speed of the precursor slurry is 20-200 g/min.
According to the embodiment of the present disclosure, the specific process parameters of the rf plasma spheroidization technique in S2 may also be: the carrier gas is argon, the carrier gas flow is 4-8L/min, the middle gas is argon, the middle gas flow is 20-30L/min, the shell gas is argon, and the shell gas flow is 70-80L/min; the feeding speed of the precursor slurry is 50-150 g/min.
According to the embodiment of the disclosure, the solvent in S1 is alcohol; the stirring speed of the mixer is 20-60 r/min, and the stirring time is 0.5-4 hours.
The spherical ferrite-based powder prepared by the method is applied to the technical field of powder injection molding or 3D printing.
Example 1:
Fe-8wt.%Cr-5wt.%Ni-1wt.%Al-2wt.%Mn-1wt.%Ti-2wt.%Mo-1wt.%Al2O3the preparation of intermetallic compound and nanometer oxide co-reinforced spherical ferrite-based powder,
atomized powder with components of Fe-8wt.% Cr-5wt.% Ni-1wt.% Al-2wt.% Mn-1wt.% Ti-2wt.% Mo and aluminum nitrate (Al (NO)3)3·9H2O) was weighed out in a mass ratio of 13.464:1 for use.
Firstly, dissolving weighed aluminum nitrate in a proper amount of alcohol, and uniformly stirring in a container to form a transparent solution. And uniformly adding the atomized powder and a proper amount of alcohol into the solution until the alloy powder is just soaked by the alcohol. And then mixed for 2 hours at a rotation speed of 40 rpm by using a mixer to obtain precursor slurry.
In the process of radio frequency plasma spheroidization, the negative pressure is 7500 Pa; the middle gas is argon, and the flow rate of the middle gas is 25L/min; the shell gas is argon, and the shell gas flow is 70L/min; argon gas with the flow rate of 4L/min is used as carrier gas, precursor solution is sprayed into a plasma arc through a feeding system and a feeding gun at the feeding speed of 150g/min, precursor slurry is instantaneously subjected to heat absorption, decomposition and melting in the plasma arc, then spheroidizing, and finally enters a cooling chamber for rapid condensation. The obtained nano oxide has an average particle size of 12.1nm, and the powder has an average particle size of 200 μm, and contains Fe-8wt.% Cr-5wt.% Ni-1wt.% Al-2wt.% Mn-1wt.% Ti-2wt.% Mo-1wt.% Al2O3The intermetallic compound and the nano-oxide co-strengthen the spherical ferrite-based powder.
Example 2:
Fe-12wt.%Cr-6wt.%Ni-1.5wt.%Al-3wt.%Mn-1.5wt.%Ti-2wt.%Mo-0.6wt.%Y2O3the preparation of intermetallic compound and nanometer oxide co-reinforced spherical ferrite-based powder,
atomized powder containing Fe-12wt.% Cr-6wt.% Ni-1.5wt.% Al-3wt.% Mn-1.5wt.% Ti-2wt.% Mo and yttrium nitrate (Y (NO)3)3·6H2O) was weighed out in a mass ratio of 48.878:1 for use.
Firstly, dissolving weighed yttrium nitrate in a proper amount of alcohol, and uniformly stirring in a container to form a transparent solution. Then evenly adding the atomized powder and a proper amount of alcohol into the solution until the alloy powderJust until it is wetted with alcohol. And then mixed for 4 hours at a rotation speed of 30 rpm by using a mixer to obtain precursor slurry. In the process of radio frequency plasma spheroidization, the negative pressure is 7800 Pa; the middle gas is argon, and the flow rate of the middle gas is 20L/min; the shell gas is argon, and the shell gas flow is 75L/min; argon gas with the flow rate of 6L/min is used as carrier gas, precursor solution is sprayed into a plasma arc through a feeding system and a feeding gun at the feeding speed of 100g/min, precursor slurry is instantaneously subjected to heat absorption, decomposition and melting in the plasma arc, then spheroidizing, and finally enters a cooling chamber for rapid condensation. The obtained nano-oxide has an average particle size of 10.2nm, powder has an average particle size of 150 μm, and Fe-12wt.% Cr-6wt.% Ni-1.5wt.% Al-3wt.% Mn-1.5wt.% Ti-2wt.% Mo-0.6wt.% Y2O3The intermetallic compound and the nano-oxide co-strengthen the spherical ferrite-based powder.
Example 3:
Fe-10wt.%Cr-7wt.%Ni-2wt.%Al-3wt.%Mn-2wt.%Ti-2wt.%Mo-0.3wt.%Y2O3the preparation of intermetallic compound and nanometer oxide co-reinforced spherical ferrite-based powder,
atomized powder with the components of Fe-10wt.% Cr-7wt.% Ni-2wt.% Al-3wt.% Mn-2wt.% Ti-3wt.% Mo and yttrium nitrate (Y (NO)3)3·6H2O) was weighed out in a mass ratio of 98.051:1 for use.
Firstly, dissolving weighed yttrium nitrate in a proper amount of alcohol, and uniformly stirring in a container to form a transparent solution. And uniformly adding the atomized powder and a proper amount of alcohol into the solution until the alloy powder is just soaked by the alcohol. And then mixed for 0.5 hour at a rotation speed of 60 rpm using a mixer to obtain precursor slurry.
In the process of radio frequency plasma spheroidization, the negative pressure is 8500 Pa; the middle gas is argon, and the flow rate of the middle gas is 22L/min; the shell gas is argon, and the shell gas flow is 78L/min; argon gas with the flow rate of 7L/min is used as carrier gas, precursor solution is sprayed into a plasma arc through a feeding system and a feeding gun at the feeding speed of 80g/min, precursor slurry is instantaneously subjected to heat absorption, decomposition and melting in the plasma arc, then spheroidizing, and finally enters a cooling chamber for rapid condensation. The resulting nano-oxide having an average particle size of 9.3nm, powder having an average particle size of 100 μm Fe-10wt.% Cr-7wt.% Ni-2wt.% Al-3wt.% Mn-2wt. -% ]Ti-2wt.%Mo-0.3wt.%Y2O3The intermetallic compound and the nano-oxide co-strengthen the spherical ferrite-based powder.
Example 4:
Fe-9wt.%Cr-8wt.%Ni-3wt.%Al-3wt.%Mn-2wt.%Ti-4wt.%Mo-0.1wt.%La2O3the preparation of intermetallic compound and nanometer oxide co-reinforced spherical ferrite-based powder,
atomized powder with the components of Fe-9wt.% Cr-8wt.% Ni-3wt.% Al-3wt.% Mn-2wt.% Ti-4wt.% Mo and lanthanum nitrate (La (NO)3)3·6H2O) was weighed out in a mass ratio of 376.067:1 for use.
Firstly, dissolving weighed lanthanum nitrate in a proper amount of alcohol, and uniformly stirring in a container to form a transparent solution. And uniformly adding the atomized powder and a proper amount of alcohol into the solution until the alloy powder is just soaked by the alcohol. And then mixed for 4 hours at a rotation speed of 20 rpm by using a mixer to obtain precursor slurry.
In the process of radio frequency plasma spheroidization, the negative pressure is 9000 Pa; the middle gas is argon, and the flow rate of the middle gas is 25L/min; the shell gas is argon, and the shell gas flow is 80L/min; argon gas with the flow rate of 8L/min is used as carrier gas, precursor solution is sprayed into a plasma arc through a feeding system and a feeding gun at the feeding speed of 50g/min, precursor slurry is instantaneously subjected to heat absorption, decomposition and melting in the plasma arc, then spheroidizing, and finally enters a cooling chamber for rapid condensation. The obtained nano oxide has an average particle size of 8.6nm, and the powder has an average particle size of 50 μm, and contains Fe-9wt.% Cr-8wt.% Ni-3wt.% Al-3wt.% Mn-2wt.% Ti-4wt.% Mo-0.1wt.% La2O3The intermetallic compound and the nano-oxide co-strengthen the spherical ferrite-based powder.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions and substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (7)
1. A method for the production of a spherical ferrite-based powder, characterized in that the method comprises the steps of,
s1, preparing precursor slurry: dissolving a nano oxide source in a proper amount of solvent to obtain a transparent solution, adding gas atomized powder into the transparent solution for completely soaking, and uniformly stirring by using a mixer to obtain uniformly mixed precursor slurry; the nano oxide source is Al (NO)3)3·9H2O、Y(NO3)3·6H2O and La (NO)3)3·6H2One of O; the addition amount of the nano oxide source ensures that the nano oxide accounts for 0.01-5 wt% of the total mass in the finally obtained spherical ferrite-based powder;
the gas atomization powder comprises the following components in percentage by mass: cr: 6-14wt.%, Ni: 3-10wt.%, Al: 1-3wt.%, Mn: 0.5-4wt.%, Ti: 1-4wt.%, Mo: 1-5wt.%, balance Fe;
s2, preparing spherical ferrite-based powder: s1, preparing the obtained precursor slurry into spherical ferrite-based powder by adopting a radio frequency plasma spheroidization technology, wherein the average particle size of an oxide dispersed phase in the spherical ferrite-based powder is less than or equal to 15 nm.
2. The method according to claim 1, wherein each component of the aerosolized powder in the s1. further comprises: cr: 8-12 wt.%, Ni: 4-8 wt.%, Al: 1-2 wt.%, Mn: 2-3 wt.%, Ti: 2-3 wt.%, Mo: 2-4wt.%, the balance being Fe.
3. The method according to claim 2, characterized in that the source of nano-oxides in said s1. is added in an amount ensuring 0.1-1wt.% of nano-oxides in the final spherical ferrite-based powder as a percentage of the total mass.
4. The method according to claim 1, wherein the specific process parameters of the rf plasma spheroidization technique in s2. are: the carrier gas is argon, and the flow rate of the carrier gas is 1-10L/min; the middle gas is argon, and the flow rate of the middle gas is 15-40L/min; the shell gas is argon, and the shell gas flow is 65-100L/min; the feeding speed of the precursor slurry is 20-200 g/min.
5. The method of claim 1, wherein the specific process parameters of the rf plasma spheroidizing technique in S2 are further: the carrier gas is argon, the carrier gas flow is 4-8L/min, the middle gas is argon, the middle gas flow is 20-30L/min, the shell gas is argon, and the shell gas flow is 70-80L/min; the feeding speed of the precursor slurry is 50-150 g/min.
6. The method according to claim 1, wherein the solvent in S1 is alcohol; the stirring speed of the mixer is 20-60 r/min, and the stirring time is 0.5-4 hours.
7. Application of the spherical ferrite-based powder prepared by the method of any one of claims 1 to 6 in the technical field of powder injection molding or 3D printing.
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